CN108102291A - A kind of light flame-retardant phenolic foam material and preparation method thereof - Google Patents
A kind of light flame-retardant phenolic foam material and preparation method thereof Download PDFInfo
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/12—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent
- C08J9/14—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent organic
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G8/00—Condensation polymers of aldehydes or ketones with phenols only
- C08G8/28—Chemically modified polycondensates
- C08G8/30—Chemically modified polycondensates by unsaturated compounds, e.g. terpenes
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- C08J2203/00—Foams characterized by the expanding agent
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- C08J2361/00—Characterised by the use of condensation polymers of aldehydes or ketones; Derivatives of such polymers
- C08J2361/04—Condensation polymers of aldehydes or ketones with phenols only
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- C08J2361/14—Modified phenol-aldehyde condensates
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- C08K7/00—Use of ingredients characterised by shape
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Abstract
The present invention relates to a kind of light flame-retardant phenolic foam materials and preparation method thereof, belong to thermal insulation material technical field.The present invention is reacted to a part for polymer architecture using the double bond participation in flax oil molecule, modified phenolic resin curing object is made to show interpenetrating polymer networks structure, effectively improve the heat resistance and thermal stability of phenolic resin, and wrap titanium diboride, redox reaction is occurred with oxygen-containing gas at high temperature by titanium diboride, by C the and O element absorptions in cracked gas and is converted into amorphous carbon and TiO2Wait solid products, inhibit a greater degree of oxicracking of resin matrix, it is embedded in simultaneously as reinforcement in the skeleton of phenol formaldehyde foam, make the compactness of skeleton increase, enhance the globality of phenol formaldehyde foam high-temperature split product, increase the residual heavy and intensity after composite material Pintsch process, hence it is evident that the fire-retardant and fire protecting performance of reinforcing material.
Description
Technical field
The present invention relates to a kind of light flame-retardant phenolic foam materials and preparation method thereof, belong to thermal insulation material technical field.
Background technology
Phenol formaldehyde foam is using phenolic resin as matrix, adds in curing agent, surfactant, foaming agent and other auxiliary agents,
While resin solidification, the gas foamed material that is dispersed therein and is formed that foaming agent is generated.Phenolic foam is opened
Hair is started from the 1940s, away from the present in existing more than 70 years.Because it is with fire-retardant, low cigarette, self-extinguishment, dimensionally stable, the burning hot decomposition of chance
The performance of the uniqueness such as pernicious gas is not discharged, and fire protecting performance is much better than other various foamed plastics, and the harm that can make fire is big
It is big to reduce, especially it is known as " king of thermal insulation material " with excellent thermal and insulating performance.Its composite foam material is largely used
In the stringent wall of the fire protection requirements such as aircraft, ship, vehicle, tunnel, oil well, mine, plate, component etc., but because it produces work
Skill is complicated, and material stability is poor in production process, its development speed of the reasons such as shock resistance and antibody Monoclonal energy force difference far away from
The foamed plastics such as polystyrene, polyethylene, polyurethane.
Meanwhile the fire incident triggered in recent years by thermal insulation material takes place frequently, the life and property to the people cause huge
Loss.Therefore country proposes more strict requirements to the thermal stability and flame retardant property of foamed material, and phenol formaldehyde foam is because of it
Flame-proof heat-resistant, smoke density and smoke toxicity are low, flame resistant penetrates, meet fire without dripping off, thermostabilization is good, chemical-resistant reagent box organic solvent
The advantages that and gradually receive significant attention.Phenolic foam is a kind of self-flame-retardant foamed plastics, in combustion will not
It melts, will not also generate stream drop, low cigarette and low toxicity characteristic.Recent domestic has developed continuous foamed molding machine,
It is contemplated that phenolic foam protruded by it fire retardant, low cigarette, low toxicity characteristic and heat resistance the advantages that, will be in building industry
It will be more widely applied as preferable heat insulation structural material.Research is suitable for the cooperative flame retardant system of phenol formaldehyde foam,
The phenolic aldehyde foam thermal insulation material of high flame resistance is developed, to realizing energy-saving and emission-reduction, the strategy of sustainable development is realized, protects numerous people
The life of the people has positive social effect with property safety.
The content of the invention
Present invention mainly solves the technical issues of：For common phenolic foam material shock resistance and antibody Monoclonal ability
Difference, the problem of fire resistance is poor, the present invention provides a kind of light flame-retardant phenolic foam materials and preparation method thereof.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention：
A kind of light flame-retardant phenolic foam material, which is characterized in that including following raw materials：
100~200 parts of phenol-formaldehyde resin modifieds, 10~20 parts of modification infusorial earths, 4~8 parts of Tween-80s, 3~6 parts of curing agent, 10~
20 parts of pentanes.
The phenol-formaldehyde resin modified reacts in acid condition for phenol with linseed oil is made linseed oil-phenol performed polymer,
It reacts generation resin in alkaline conditions with formaldehyde again, and wraps up titanium diboride and be made.
The phenol, linseed oil, the mass ratio of formaldehyde are 9：10：5.4, the titanium diboride dosage is phenol quality
5%。
The acid condition is that mass fraction is added dropwise is 20% salt acid for adjusting pH to 3~5.
The alkaline condition be with mass fraction be 20% sodium hydroxide solution adjust pH to 9~10.
The modification infusorial earth for diatomite and multi-walled carbon nanotube ultrasonic disperse in deionized water, mistake after insulation reaction
Filter washing drying is made.
The mass ratio of the diatomite and multi-walled carbon nanotube is 10：1.
The curing agent is P-TOLUENE SULFO ACID 99, phenolsulfonic acid, xylene monosulfonic acid, acetic acid, sulfuric acid, one kind in phosphoric acid or more
Kind.
The preparation method of a kind of light flame-retardant phenolic foam material, which is characterized in that concretely comprise the following steps：
（1）Diatomite, multi-walled carbon nanotube are taken, ultrasonic disperse in deionized water, is again heated to 90~100 DEG C, insulation reaction
20~for 24 hours, it filters, wash after being cooled to room temperature, is dry, obtaining modification infusorial earth；
（2）Mass fraction at 70~80 DEG C is taken to be mixed for 10% phenol solution with linseed oil, 10~15min of insulated and stirred, then use salt
Acid for adjusting pH stirs 20~30min, obtains performed polymer to 3~5；
（3）Performed polymer is added in into mass fraction as in 10% formalin, and pH to 9~10, heating are adjusted with sodium hydroxide solution
To 60~70 DEG C of 30~40min of insulation reaction, titanium diboride is added, is heated to 90~95 DEG C of 50~60min of insulation reaction, then
PH is adjusted to neutrality, obtains phenol-formaldehyde resin modified；
（4）Phenol-formaldehyde resin modified, modification infusorial earth, Tween-80, curing agent, pentane are taken, 1 is stirred with 500~1000r/min
It is poured into after~3min in foaming mould, mold is put into 50~60min of foaming on 70~80 DEG C of vulcanizing press, then is warming up to
120~150 DEG C, cure 1~2h, demoulded after being cooled to room temperature, obtain light flame-retardant phenolic foam material.
The beneficial effects of the invention are as follows：
（1）The present invention is reacted to a part for polymer architecture using the double bond participation in flax oil molecule, makes modified phenol
Urea formaldehyde solidfied material shows interpenetrating polymer networks structure, effectively improves the heat resistance and thermal stability of phenolic resin, and
Titanium diboride is wrapped, redox reaction is occurred with oxygen-containing gas by titanium diboride at high temperature, by the C in cracked gas
With O element absorptions and be converted into amorphous carbon and TiO2Solid products are waited, inhibit a greater degree of oxicracking of resin matrix, together
Shi Zuowei reinforcements are embedded in the skeleton of phenol formaldehyde foam, make the compactness of skeleton increase, and enhance phenol formaldehyde foam Pintsch process
The globality of product increases the residual heavy and intensity after composite material Pintsch process, hence it is evident that the fire-retardant and fire protecting performance of reinforcing material；
（2）The present invention utilizes diatomaceous cellular structure, during Foaming of phenolic resin, can adsorb free phenolic aldehyde and
Steam reduces the probability of bubble breaking, makes the rate of closed hole higher of abscess, and plays the effect of nucleating agent, causes abscess more equal
It is even, it is smaller so that anti-pressure ability is more preferable, and compressive strength bigger is effectively improved shock resistance and antibody Monoclonal ability, simultaneously
It is bridged by carbon nanotubes, plays the role of a kind of " sealant ", the collective effect of the two can make what is formed in combustion process
Layer of charcoal surface hole defect is reduced, and diatomaceous barrier blocking effect hinders fuel gas and oxygen further so as to play more preferably
Into raising fire resistance.
Specific embodiment
20~30g diatomite is taken, 2~3g multi-walled carbon nanotubes are added in 200~300mL deionized waters, at 60~80 DEG C
Under, 20~30min is disperseed with 200W ultrasonic echographies, is again heated to 90~100 DEG C, insulation reaction 20~for 24 hours, it is cooled to room temperature
After filter, filter residue is washed with deionized 2~3 times, then filter residue is placed in drying box, dry 10~12h at 70~80 DEG C,
Modification infusorial earth is obtained, it is 10% phenol solution to take 90~135g mass fractions at 70~80 DEG C, is mixed with 10~20g linseed oil, with
300~400r/min, 10~15min of insulated and stirred, then be added dropwise mass fraction for 20% salt acid for adjusting pH to 3~5, continue stirring 20
~30min, obtains performed polymer, and performed polymer is added in 54~81g mass fractions in 10% formalin, and is 20% with mass fraction
Sodium hydroxide solution adjusts pH to 9~10, is heated to 60~70 DEG C, 30~40min of insulation reaction adds 4.5~9.0g bis-
Titanium boride, is heated to 90~95 DEG C, 50~60min of insulation reaction, then with mass fraction is 20% salt acid for adjusting pH to neutrality, obtains
Phenol-formaldehyde resin modified takes 100~200g phenol-formaldehyde resin modifieds, 10~20g modification infusorial earths, 4~8g Tween-80s, 3~6g curings
Agent, 10~20g pentanes pour into foaming mould after stirring 1~3min with 500~1000r/min, mold are put into 70~80
DEG C vulcanizing press on foam 50~60min, then be warming up to 120~150 DEG C, cure 1~2h, demoulded after being cooled to room temperature,
Obtain light flame-retardant phenolic foam material.
Example 1
20g diatomite is taken, 2g multi-walled carbon nanotubes are added in 200mL deionized waters, at 60 DEG C, with 200W ultrasonic echographies
Scattered 20min, is again heated to 90 DEG C, and insulation reaction 20h is filtered after being cooled to room temperature, and filter residue is washed with deionized 2 times, then
Filter residue is placed in drying box, dry 10h, obtains modification infusorial earth at 70 DEG C, and it is 10% phenol to take 90g mass fractions at 70 DEG C
Solution is mixed with 10g linseed oil, with 300r/min insulated and stirred 10min, then be added dropwise mass fraction for 20% salt acid for adjusting pH extremely
3, continue to stir 20min, obtain performed polymer, performed polymer is added in into 54g mass fractions as in 10% formalin, and uses mass fraction
PH to 9 is adjusted for 20% sodium hydroxide solution, is heated to 60 DEG C, insulation reaction 30min adds 4.5g titanium diborides, is heated to
90 DEG C, insulation reaction 50min, then with mass fraction for 20% salt acid for adjusting pH to neutrality, obtain phenol-formaldehyde resin modified, 100g taken to change
Property phenolic resin, 10g modification infusorial earths, 4g Tween-80s, 3g curing agent, 10g pentanes, with 500/min stir 1min after pour into
In foaming mould, mold is put on 70 DEG C of vulcanizing press the 50min that foams, then is warming up to 120 DEG C, cures 1h, is cooled to
It is demoulded after room temperature, obtains light flame-retardant phenolic foam material.
Example 2
25g diatomite is taken, 2g multi-walled carbon nanotubes are added in 250mL deionized waters, under 70 DEG C 5, with 200W ultrasonic echographies
Scattered 25min, is again heated to 95 DEG C, and insulation reaction 22h is filtered after being cooled to room temperature, and filter residue is washed with deionized 2 times, then
Filter residue is placed in drying box, dry 11h, obtains modification infusorial earth at 75 DEG C, and it is 10% phenol to take 114g mass fractions at 75 DEG C
Solution is mixed with 15g linseed oil, with 350r/min insulated and stirred 12min, then be added dropwise mass fraction for 20% salt acid for adjusting pH extremely
4, continue to stir 25min, obtain performed polymer, performed polymer is added in into 63g mass fractions as in 10% formalin, and uses mass fraction
PH to 9.5 is adjusted for 20% sodium hydroxide solution, 65 DEG C, insulation reaction 35min is heated to, adds 6.5g titanium diborides, is heated
To 92 DEG C, insulation reaction 55min, then with mass fraction for 20% salt acid for adjusting pH to neutrality, obtain phenol-formaldehyde resin modified, take 150g
Phenol-formaldehyde resin modified, 15g modification infusorial earths, 6g Tween-80s, 4g curing agent, 15g pentanes, after stirring 2min with 750r/min
It pours into foaming mould, mold is put on 70~80 DEG C of vulcanizing press the 55min that foams, then be warming up to 135 DEG C, cure
1h is demoulded after being cooled to room temperature, and obtains light flame-retardant phenolic foam material.
Example 3
30g diatomite is taken, 3g multi-walled carbon nanotubes are added in 300mL deionized waters, at 80 DEG C, with 200W ultrasonic echographies
Scattered 30min, is again heated to 100 DEG C, and insulation reaction for 24 hours, filters after being cooled to room temperature, and filter residue is washed with deionized 3 times, then
Filter residue is placed in drying box, dry 12h, obtains modification infusorial earth at 80 DEG C, and it is 10% phenol to take 135g mass fractions at 80 DEG C
Solution is mixed with 20g linseed oil, with 400r/min insulated and stirred 15min, then be added dropwise mass fraction for 20% salt acid for adjusting pH extremely
5, continue to stir 30min, obtain performed polymer, performed polymer is added in into 81g mass fractions as in 10% formalin, and uses mass fraction
PH to 10 is adjusted for 20% sodium hydroxide solution, 70 DEG C, insulation reaction 40min is heated to, adds 9.0g titanium diborides, is heated
To 95 DEG C, insulation reaction 60min, then with mass fraction for 20% salt acid for adjusting pH to neutrality, obtain phenol-formaldehyde resin modified, take 200g
Phenol-formaldehyde resin modified, 20g modification infusorial earths, 8g Tween-80s, 6g curing agent, 20g pentanes are stirred with 1000r/min
It is poured into after 3min in foaming mould, mold is put on 80 DEG C of vulcanizing press the 60min that foams, then be warming up to 150 DEG C, cured
2h is demoulded after being cooled to room temperature, and obtains light flame-retardant phenolic foam material.
A kind of light flame-retardant phenolic foam material that the present invention is prepared into and the phenol formaldehyde foam material of Guangzhou company production
Material is detected, specific testing result such as following table table 1
1 light flame-retardant phenolic foam material performance characterization of table
As shown in Table 1, a kind of light flame-retardant phenolic foam material that the present invention is prepared into, abscess is smaller, and distribution of cells is more equal
Even, limit oxygen index is promoted, and rate of slag falling reduces, and fire resistance is significantly improved.
Claims (9)
1. a kind of light flame-retardant phenolic foam material, which is characterized in that including following raw materials：
100~200 parts of phenol-formaldehyde resin modifieds, 10~20 parts of modification infusorial earths, 4~8 parts of Tween-80s, 3~6 parts of curing agent, 10~
20 parts of pentanes.
2. a kind of light flame-retardant phenolic foam material as described in claim 1, which is characterized in that the phenol-formaldehyde resin modified is
Phenol reacts in acid condition with linseed oil is made linseed oil-phenol performed polymer, then reacts raw in alkaline conditions with formaldehyde
Resin, and wrap up titanium diboride and be made.
3. a kind of light flame-retardant phenolic foam material as claimed in claim 2, which is characterized in that the phenol, linseed oil, first
The mass ratio of aldehyde is 9：10：5.4, the titanium diboride dosage is the 5% of phenol quality.
4. a kind of light flame-retardant phenolic foam material as claimed in claim 2, which is characterized in that the acid condition is dropwise addition
Mass fraction is 20% salt acid for adjusting pH to 3~5.
5. a kind of light flame-retardant phenolic foam material as claimed in claim 2, which is characterized in that the alkaline condition is to use matter
It measures fraction and adjusts pH to 9~10 for 20% sodium hydroxide solution.
6. a kind of light flame-retardant phenolic foam material as described in claim 1, which is characterized in that the modification infusorial earth is silicon
With multi-walled carbon nanotube ultrasonic disperse in deionized water, filtration washing drying is obtained after insulation reaction for diatomaceous earth.
7. a kind of light flame-retardant phenolic foam material as claimed in claim 6, which is characterized in that the diatomite and multi wall carbon
The mass ratio of nanotube is 10：1.
8. a kind of light flame-retardant phenolic foam material as described in claim 1, which is characterized in that the curing agent is to benzene sulphur
One or more in acid, phenolsulfonic acid, xylene monosulfonic acid, acetic acid, sulfuric acid, phosphoric acid.
9. a kind of preparation method of light flame-retardant phenolic foam material as described in claim 1~8 any one, feature exist
In concretely comprising the following steps：
（1）Diatomite, multi-walled carbon nanotube are taken, ultrasonic disperse in deionized water, is again heated to 90~100 DEG C, insulation reaction
20~for 24 hours, it filters, wash after being cooled to room temperature, is dry, obtaining modification infusorial earth；
（2）Mass fraction at 70~80 DEG C is taken to be mixed for 10% phenol solution with linseed oil, 10~15min of insulated and stirred, then use salt
Acid for adjusting pH stirs 20~30min, obtains performed polymer to 3~5；
（3）Performed polymer is added in into mass fraction as in 10% formalin, and pH to 9~10, heating are adjusted with sodium hydroxide solution
To 60~70 DEG C of 30~40min of insulation reaction, titanium diboride is added, is heated to 90~95 DEG C of 50~60min of insulation reaction, then
PH is adjusted to neutrality, obtains phenol-formaldehyde resin modified；
（4）Phenol-formaldehyde resin modified, modification infusorial earth, Tween-80, curing agent, pentane are taken, 1 is stirred with 500~1000r/min
It is poured into after~3min in foaming mould, mold is put into 50~60min of foaming on 70~80 DEG C of vulcanizing press, then is warming up to
120~150 DEG C, cure 1~2h, demoulded after being cooled to room temperature, obtain light flame-retardant phenolic foam material.
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| CN104356591A (en) * | 2014-11-06 | 2015-02-18 | 聊城大学 | Toughened enhanced phenolic foam insulation material and preparation method thereof |
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2017
- 2017-12-12 CN CN201711316859.3A patent/CN108102291A/en active Pending
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|---|---|---|---|---|
| JPH03122070A (en) * | 1989-10-04 | 1991-05-24 | Chuo Shirika Kk | Method for forming active carbon layer in foamed ceramics or diatomaceous earth |
| CN103013038A (en) * | 2012-12-27 | 2013-04-03 | 北京莱恩斯高新技术有限公司 | Cardanol modified phenolic aldehyde foam and preparation method thereof |
| CN104072940A (en) * | 2014-07-03 | 2014-10-01 | 中国科学院合肥物质科学研究院 | Nano titanium nitride-phenolic aldehyde composite foam material and preparation method thereof |
| CN104356591A (en) * | 2014-11-06 | 2015-02-18 | 聊城大学 | Toughened enhanced phenolic foam insulation material and preparation method thereof |
| CN106243613A (en) * | 2016-08-01 | 2016-12-21 | 合肥广能新材料科技有限公司 | Phenol formaldehyde foam thermal insulating composite panel and preparation method thereof |
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| Title |
|---|
| 刘天祥等: "TiB2增强酚醛泡沫的制备及性能", 《工程塑料应用》 * |
| 康义: "《有色金属工业绿色发展循环发展低碳发展：中国有色金属学会第九届学术年会论文集》", 30 September 2013, 中南大学出版社 * |
| 袁莉莉等: "羧基碳纳米管增强酚醛泡沫的压缩性能及热性能", 《复合材料学报》 * |
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